US11437217B2 - Method for preparing a sample for transmission electron microscopy - Google Patents

Method for preparing a sample for transmission electron microscopy Download PDF

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US11437217B2
US11437217B2 US17/332,114 US202117332114A US11437217B2 US 11437217 B2 US11437217 B2 US 11437217B2 US 202117332114 A US202117332114 A US 202117332114A US 11437217 B2 US11437217 B2 US 11437217B2
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layer
patterned
area
target area
contrasting material
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US20210391144A1 (en
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Eric Vancoille
Niels Bosman
Patrick Carolan
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Interuniversitair Microelektronica Centrum vzw IMEC
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/26—Electron or ion microscopes; Electron or ion diffraction tubes
    • H01J37/261—Details
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
    • G01N23/2202—Preparing specimens therefor
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/30—Electron-beam or ion-beam tubes for localised treatment of objects
    • H01J37/305—Electron-beam or ion-beam tubes for localised treatment of objects for casting, melting, evaporating, or etching
    • H01J37/3053—Electron-beam or ion-beam tubes for localised treatment of objects for casting, melting, evaporating, or etching for evaporating or etching
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/04—Coating on selected surface areas, e.g. using masks
    • C23C16/045—Coating cavities or hollow spaces, e.g. interior of tubes; Infiltration of porous substrates
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/06—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of metallic material
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/48—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating by irradiation, e.g. photolysis, radiolysis, particle radiation
    • C23C16/487—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating by irradiation, e.g. photolysis, radiolysis, particle radiation using electron radiation
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/32—Polishing; Etching
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/02—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material
    • G01N23/04—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material and forming images of the material
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/30—Electron-beam or ion-beam tubes for localised treatment of objects
    • H01J37/317—Electron-beam or ion-beam tubes for localised treatment of objects for changing properties of the objects or for applying thin layers thereon, e.g. for ion implantation
    • H01J37/3178—Electron-beam or ion-beam tubes for localised treatment of objects for changing properties of the objects or for applying thin layers thereon, e.g. for ion implantation for applying thin layers on objects
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/2813—Producing thin layers of samples on a substrate, e.g. smearing, spinning-on
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/26—Electron or ion microscopes
    • H01J2237/262—Non-scanning techniques
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/26—Electron or ion microscopes
    • H01J2237/28—Scanning microscopes
    • H01J2237/2802—Transmission microscopes

Definitions

  • the present application is related to the field of transmission electron microscopy (TEM), and in particular, to methods for preparing a TEM sample for visualizing nano-scaled structures, as produced in semiconductor processing.
  • TEM transmission electron microscopy
  • TEM Transmission electron microscopy
  • FIB focused ion beam milling
  • a mask and a protective layer are needed. This protective layer can be applied by a variety of methods.
  • samples with a polymeric top surface are prone to damage by any of the methods mentioned above and/or do not exhibit enough contrast with the protective layer to be distinguished during TEM observations.
  • Depositing an additional contrasting layer by, for example, sputtering techniques is not an option in the case of vulnerable structures such as polymer resist lines or porous silicon structures because sputtering techniques tend to damage the structures.
  • a substrate disclosed herein comprises a patterned area on its surface defined by a given topography of nano-sized features, for example, a set of parallel polymer resist lines.
  • the substrate is configured to facilitate extraction of a TEM sample in the form of a slice of the substrate cut out transversally to the substrate surface.
  • the TEM sample facilitates visualizing the topography by TEM.
  • a thin conformal layer of contrasting material is deposited on the topography by depositing a thicker layer of the contrasting material on a local target area of the substrate that is spaced apart from the patterned area, i.e., located at a non-zero distance from the patterned area.
  • the material deposited on the target area is deposited by Electron Beam Induced Deposition (EBID), and in an example, without using a mask to cover the substrate surface outside the local target area.
  • EBID Electron Beam Induced Deposition
  • a conformal layer of the contrasting material is formed on the topography of the patterned area.
  • the conformal layer follows the topography and does not fill spaces between adjacent features of the topography.
  • the protective layer which does not damage the topography in the patterned area as it is protected by the conformal layer.
  • the TEM sample is processed further in subsequent operations, for example, by FIB.
  • the contrast provided between the conformal contrasting layer and the protective layer facilitates the performance of high-quality TEM analysis.
  • An aspect of the disclosure relates to a method for preparing a TEM sample that facilitates the performance of TEM.
  • the method comprises:
  • the features of the patterned area are formed of a polymer, and the contrasting material is a heavy metal, for example, Pt.
  • the contrasting material is deposited in a single target area, and the thickness of the conformal layer decreases as a function of the distance to the target area.
  • the contrasting material is deposited in two or more target areas, and the conformal layer is at least partially formed by the addition of conformal layers formed as a consequence of the deposition of the contrasting material in the two or more target areas.
  • An aspect also relates to the use of EBID for depositing a layer of a contrasting material on a patterned area comprising pattern features that define a topology by depositing a layer of the contrasting material locally in at least one target area spaced apart from the patterned area, in such a manner that a portion of the contrasting material is also deposited around the target area, thereby forming a conformal layer of the contrasting material on at least some of the features in the patterned area.
  • the conformal layer is suitable as a contrasting layer when producing a TEM sample of the patterned area.
  • FIG. 1 shows a front view and a top view of an array of polymer resist lines on a substrate, in accordance with an example embodiment.
  • FIG. 2 illustrates the local Pt deposition and conformal Pt layer deposition on the substrate of FIG. 1 , in accordance with an example embodiment.
  • FIGS. 3 a and 3 b illustrate a detail of the conformal layer on the array of resist lines, before and after deposition of a spin-on carbon layer, for the case of a single Pt deposition to one side of the resist lines, in accordance with an example embodiment.
  • FIG. 4 illustrates two local depositions are performed, one on either side of the array of resist lines, in accordance with an example embodiment.
  • FIGS. 5 a and 5 b illustrate a detail of the conformal layer on the array of resist lines before and after deposition of a spin-on carbon layer for the case of two Pt depositions, in accordance with an example embodiment.
  • FIG. 1 shows a substrate 1 .
  • An example of the substrate 1 is a glass substrate with a layer of silicon 2 on its surface.
  • a patterned area 8 is disposed on the Si layer.
  • the patterned area 8 comprises an array of parallel polymer resist lines 3 that, in an example, are produced by a lithographic patterning technique.
  • the width (measured in the plane of the drawing) and height of the lines 3 are on the order of nanometers, for example, between 10 and 20 nanometers.
  • the pitch of the array of lines is of the same order of magnitude.
  • the aim is obtaining a TEM sample that allows the verification of these dimensions.
  • a protective spin-on carbon (SoC) layer is to be deposited on the resist lines 3 , and a TEM sample of the substrate is to be produced in a focused ion beam (FIB) tool by milling away material on either side of a thin slice oriented in the direction perpendicular to the lines 3 .
  • An outline of the sample 4 is indicated in the top view of FIG. 1 . According to an aspect, however, an additional step is performed prior to depositing the SoC layer.
  • a layer 5 of platinum having a thickness T is deposited locally in a rectangular target area 6 to one side of the array of resist lines 3 , spaced apart from the array by a distance D, the distance D extending in a transversal direction relative to the lines 3 , in this case, perpendicular to the lines.
  • the local deposition is performed by Electron Beam Induced Deposition (EBID), and in an example, is performed in the FIB tool that is to be used for producing the TEM sample.
  • EBID Electron Beam Induced Deposition
  • a thin layer 7 of the deposited material is also produced in a region surrounding the target area 6 .
  • the thin layer is a result of the generation of secondary and backscattered electrons in the polymer material of the lines 3 and in the deposited material itself.
  • Careful selection of the distance D, the thickness T of the Pt in the target area 6 , and the deposition parameters applied in the EBID process facilitates conformally forming the thin layer 7 on the resist lines 3 , i.e., the layer follows the topography defined by the lines 3 and does not fill the spaces between two adjacent lines 3 .
  • the conformal layer 7 does not damage the polymer lines 3 , given the fact that the conformal layer 7 is formed outside the area 6 that is directly affected by the EBID process.
  • the conformal layer 7 has a thickness of a few nanometers, which decreases gradually as a function of the distance from the target area 6 .
  • the distance D and the thickness T are chosen as a function of the dimensions of the array of lines 3 (height and width of the lines and pitch of the array), so that all the lines 3 of the array receive a contrast layer that is detectable by TEM.
  • the parameters D and T and other deposition parameters may, therefore, depend on the exact dimensions of the patterned area 8 and of the features within the area. A limited number of trials is, however, sufficient for finding a suitable set of deposition parameters.
  • a layer 10 of spin-on carbon (SoC) is then deposited on top of the Pt layer 7 to serve as the protective layer required during the TEM sample processing.
  • the protective layer could be another suitable material known in the art, applied by any technique known for this purpose.
  • the substrate is then moved back to the FIB tool for producing the TEM sample 4 .
  • the TEM image obtainable from the sample 4 corresponds to the section view shown in FIG. 3 b .
  • the conformal layer 7 does not have a constant thickness, the conformal layer 7 provides a clear contrast between the lines 3 and the SoC layer 10 , and thereby permits the lines 3 to be clearly visualized in the TEM image so that the dimensions of the lines can be measured and/or verified.
  • the Pt layer 7 protects the polymer lines 3 from any damage during the deposition of the SoC layer 10 .
  • the deposition by EBID is applied only to the target area 6 , i.e., not directly to the area of interest 8 , thereby avoiding possible damage to the polymer lines 3 caused by the high electron currents applied in the EBID process.
  • FIG. 4 shows an embodiment wherein local Pt layers 5 a and 5 b of equal thickness T are deposited on both sides of the patterned area 8 comprising the array of polymer resist lines 3 , in two equal-sized rectangular target areas 6 a and 6 b , placed at equal distance D from the array.
  • the layers 5 a and 5 b are applied sequentially, i.e., through deposition by EBID in area 6 a followed by area 6 b or vice versa.
  • the decreasing thicknesses of the conformal Pt layers 7 a and 7 b resulting from the two Pt depositions now add up and form a contrast layer with a substantially constant thickness, as shown in the detail images in FIGS. 5 a and 5 b .
  • the image obtained from the TEM sample 4 now resembles the view shown in FIG. 5 b .
  • the contrast layer 7 a + 7 b has a substantially constant thickness across the array of resist lines 3 .
  • the combined conformal layer 7 a + 7 b could have a higher thickness on the outer lines than in the middle of the array, this lower thickness, however, being sufficient to provide the required contrast. It is also possible to deposit layer 5 a at a different distance from the array 8 than the layer 5 b , for example, if the available space for the target areas is not the same on both sides of the array. In that case, the thickness T of the layers 5 a and 5 b could be different in order to ensure that a conformal layer of suitable thickness is eventually formed on the lines 3 .
  • more than two layers 5 a , 5 b , 5 c , etc. could be deposited sequentially in more than two respective target areas 6 a , 6 b , 6 c , etc., if the size and other characteristics of the patterned area would require this.
  • the in-plane shape of the target 6 or areas 6 a , 6 b , etc. could be other than the rectangular shape illustrated in the drawings. If the contrast layer 7 (or 7 a + 7 b + . . .
  • the thickness T and/or the distance D and possibly other parameters could be adapted so that the contrast layer 7 is at least deposited on the sub-area of the patterned area 8 .
  • the method allows a degree of flexibility as a function of the characteristics of the structure of which a TEM sample is required.
  • EBID parameters are suitable for obtaining a contrasting layer of Pt on an array of polymer resist lines like the array illustrated in the drawings, the width of the lines, measured perpendicular to the longitudinal direction of the lines, being about 14 nm, the height about 15 nm, the pitch about 30 nm.
  • Examples of the in-plane dimensions of the Pt target areas 6 are 0.3 ⁇ m ⁇ 2 ⁇ m.
  • the in-plane dimensions may be chosen depending on local structure features.
  • the aspects disclosed herein are not limited to any of the materials cited above.
  • the aspects are primarily useful for producing TEM samples comprising features of a vulnerable material such as polymer or porous silicon, and/or a material that shows little or no contrast with the protective layer required for the TEM sample preparation.
  • the contrast layer may be formed of any material that is not reactive with the material of the features that are to be imaged by TEM.
  • other heavy metals besides Pt are suitable as materials for the contrast layer, e.g., W, Hf, Mo, Au, Ir, etc., which can be deposited in a FIB instrument using an appropriate chemical precursor and the EBID mode.
  • the structure that is to be imaged may be any patterned structure defined by a given topography.
  • the aspects disclosed herein are applicable, for example, to all scaled structures and stacks used in patterning where the top is a resist, or a structure with complex layers of resist as used in DSA (Directed Self-Assembly), SADP/SAQP (Self-Aligned Double and Quadruple Patterning) methods, or a structure where analysis of a polymeric activation layer for selective deposition is required.
  • DSA Directed Self-Assembly
  • SADP/SAQP Self-Aligned Double and Quadruple Patterning

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EP20179637.2A EP3922752B1 (de) 2020-06-12 2020-06-12 Verfahren zur herstellung einer probe für die transmissionselektronenmikroskopie
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CN114354664A (zh) * 2022-01-10 2022-04-15 长江存储科技有限责任公司 使用fib制备截面样品的方法和截面样品的观察方法

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